(S)-2-(Boc-氨基)-3-[(S)-2-氧代-3-吡咯烷基]丙酸甲酯单晶制备及其结构表征

Single crystal culture and its structure characterization of methyl(S)-2-(tert�butoxycarbonyl)amino-3-[(S)-2-oxopyrrolidin-3-yl]propanoate

目的培养(S)-2-(Boc-氨基)-3-[(S)-2-氧代-3-吡咯烷基]丙酸甲酯单晶,并进行晶型表征和立体结构确证。方法用醋酸乙酯–甲基叔丁基醚(1∶1)体系培养单晶,并采用热重法、差示扫描量热法、粉末X射线衍射和单晶X射线衍射分析。结果制备得到无色块状晶体;样品熔点约为114℃;该晶胞属于正交晶系,空间群为P2_(1)2_(1)2_(1),分子式为C_(13)H_(22)N2O_(5),相对分子质量为286.33,晶体密度为1.152 mg/mm^(3),绝对构型为S,S构型。结论确定了(S)-2-(Boc-氨基)-3-[(S)-2-氧代-3-吡咯烷基]丙酸甲酯的立体构型,培养的晶体为非水合物和溶剂化物。

Objective To cultivate the single crystal and perform crystal morphology characterization and stereo-structural confirmation of methyl(S)-2-(tert-butoxycarbonyl)amino-3-[(S)-2-oxopyrrolidin-3-yl]propanoate.Methods The single crystals were cultivated with of ethyl acetate-methyl tert-butyl ether(1∶1)solvent system,and TGA,DSC,XRPD,and SXRD were used to analyze.Results Nice colorless bulk crystals were obtained with approximately 114℃of melting point.The crystal cell belongs to an orthogonal crystal system,with a spatial group of P2_(1)2_(1)2_(1).Molecular formula was C_(13)H_(22)N_(2)O_(5),molecular weight was 286.33,crystal density was 1.152 mg/mm^(3),and an absolute configuration was S,S style.Conclusion The stereo-configuration of methyl(S)-2-(tert-butoxycarbonyl)amino-3-[(S)-2-oxopyrrolidin-3-yl]propanoate has been confirmed,and the cultured crystals are non-hydrated and solvated.